联二脲

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 360 g of hydrazodicarbonamide, 807 g of stearyl amine and 1 ml of tin(II)dioctoate are stirred in 1 liter of N-methyl pyrrolidone for 4 hours at 175° C. and for 6 hours at 200° C. A deposit precipitates on cooling and is isolated by filtration under suction and washed with water, giving 955 g (90% of the theoretical) of 4-stearyl-1,2,4-triazolidine-3,5-dione in the form of colourless crystals melting at 118° to 120° C. A deposit precipitates on cooling is isolated by filtration under suction washed with water

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 64.2 g of hydrazodicarbonamide and 37 g of m-xylylene diamine in 300 ml of N-methyl pyrrolidone are heated with stirring for 4 hours to 175° C. and for 30 hours to 200° C. The solvent is then distilled off in vacuo and the residue is recrystallised from chloroform, giving 58 g (70% of the theoretical) of 1,3-bis-(1,2,4-triazolidine-3,5-dione-4-yl-methyl)-benzene in the form of colourless crystals melting at 244° to 246° C. The solvent is then distilled off in vacuo the residue is recrystallised from chloroform

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 765 g of 1-aminomethyl-5-amino-1,3,3-trimethyl cyclohexane and 708 g of hydrazodicarbonamide are stirred in 1 liter of N-methyl pyrrolidone for 4 hours at 175° C., for 5 hours at 200° C. and for 15 hours at 220° C. The solvent is then distilled off in vacuo and the residue is dried in vacuo, giving 1473 g (97% of the theoretical) of 1-(3,5-dioxo-1,2,4-triazolidin-4-yl-methyl)-1,3,3-trimethyl-5-(3,5-dioxo-1,2,4-triazolidin-4-yl)-cyclohexane in the form of colourless crystals melting at 213 C. (decomposition). The solvent is then distilled off in vacuo the residue is dried in vacuo

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 765 g of 1-aminomethyl-5-amino-1,3,3-trimethyl cyclohexane and 708 g of hydrazodicarbonamide are stirred in 1 liter of N-methyl pyrrolidone for 4 hours at 175° C., for 5 hours at 200° C. and for 15 hours at 220° C. The solvent is then distilled off in vacuo and the residue is dried in vacuo, giving 1473 g (97% of the theoretical) of 1-(3,5-dioxo-1,2,4-triazolidin-4-yl-methyl)-1,3,3-trimethyl-5-(3,5-dioxo-1,2,4-triazolidin-4-yl)-cyclohexane in the form of colourless crystals melting at 213 C. (decomposition). The solvent is then distilled off in vacuo the residue is dried in vacuo

反应条件: temp:2.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A stirred suspension of allyl isothiocyanate (19.8 g, 0.2 mole) and of 4-methyl-3-thiosemicarbazide (21.0 g, 0.2 mole) in 150 ml denatured ethanol (5% methanol) was refluxed for one hour. The crystalline suspension was briefly chilled, and the 1-allyl-6-methyl-2,5-dithiobiurea was collected and vacuum dried. A stirred solution of this biurea (30.6 g, 0.15 mole) in phosphorous oxychloride (150 ml) was refluxed for 11/2 hours. Unreacted phosphorus oxychloride was removed in vacuo, and the residue carefully partitioned between 1.2 M hydrochloric acid (150 ml) and chloroform (150 ml) while maintaining this mixture at 2° C with ice-bath cooling. The chloroform phase was extracted with another portion of 1.2 M hydrochloric acid (100 ml), and the combined acid layer was carefully made alkaline with conc. ammonium hydroxide. The resultant alkaline suspension was extracted with two portions of chloroform, and the combined chloroform extract was washed with a small portion of distilled water. After drying this chloroform extract over magnesium sulfate, the solvent was removed under reduced pressure to yield a colorless solid. Crystallization of the product from ethyl acetate gave 7.3 g (29 percent) of 2-allylamino-5-methylamino-1,3,4-thiadiazole (a colorless solid). Analysis confirmed the desired product. was refluxed for one hour The crystalline suspension was briefly chilled the 1-allyl-6-methyl-2,5-dithiobiurea was collected vacuum dried was removed in vacuo the residue carefully partitioned between 1.2 M hydrochloric acid (150 ml) and chloroform (150 ml) cooling The chloroform phase was extracted with another portion of 1.2 M hydrochloric acid (100 ml) The resultant alkaline suspension was extracted with two portions of chloroform the combined chloroform extract was washed with a small portion of distilled water After drying this chloroform extract over magnesium sulfate the solvent was removed under reduced pressure to yield a colorless solid Crystallization of the product from ethyl acetate

反应条件: temp:2.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A stirred suspension of allyl isothiocyanate (19.8 g, 0.2 mole) and of 4-methyl-3-thiosemicarbazide (21.0 g, 0.2 mole) in 150 ml denatured ethanol (5% methanol) was refluxed for one hour. The crystalline suspension was briefly chilled, and the 1-allyl-6-methyl-2,5-dithiobiurea was collected and vacuum dried. A stirred solution of this biurea (30.6 g, 0.15 mole) in phosphorous oxychloride (150 ml) was refluxed for 11/2 hours. Unreacted phosphorus oxychloride was removed in vacuo, and the residue carefully partitioned between 1.2 M hydrochloric acid (150 ml) and chloroform (150 ml) while maintaining this mixture at 2° C with ice-bath cooling. The chloroform phase was extracted with another portion of 1.2 M hydrochloric acid (100 ml), and the combined acid layer was carefully made alkaline with conc. ammonium hydroxide. The resultant alkaline suspension was extracted with two portions of chloroform, and the combined chloroform extract was washed with a small portion of distilled water. After drying this chloroform extract over magnesium sulfate, the solvent was removed under reduced pressure to yield a colorless solid. Crystallization of the product from ethyl acetate gave 7.3 g (29 percent) of 2-allylamino-5-methylamino-1,3,4-thiadiazole (a colorless solid). Analysis confirmed the desired product. was refluxed for one hour The crystalline suspension was briefly chilled the 1-allyl-6-methyl-2,5-dithiobiurea was collected vacuum dried was removed in vacuo the residue carefully partitioned between 1.2 M hydrochloric acid (150 ml) and chloroform (150 ml) cooling The chloroform phase was extracted with another portion of 1.2 M hydrochloric acid (100 ml) The resultant alkaline suspension was extracted with two portions of chloroform the combined chloroform extract was washed with a small portion of distilled water After drying this chloroform extract over magnesium sulfate the solvent was removed under reduced pressure to yield a colorless solid Crystallization of the product from ethyl acetate

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 360 g of hydrazodicarbonamide, 807 g of stearyl amine and 1 ml of tin(II)dioctoate are stirred in 1 liter of N-methyl pyrrolidone for 4 hours at 175° C. and for 6 hours at 200° C. A deposit precipitates on cooling and is isolated by filtration under suction and washed with water, giving 955 g (90% of the theoretical) of 4-stearyl-1,2,4-triazolidine-3,5-dione in the form of colourless crystals melting at 118° to 120° C. A deposit precipitates on cooling is isolated by filtration under suction washed with water

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 765 g of 1-aminomethyl-5-amino-1,3,3-trimethyl cyclohexane and 708 g of hydrazodicarbonamide are stirred in 1 liter of N-methyl pyrrolidone for 4 hours at 175° C., for 5 hours at 200° C. and for 15 hours at 220° C. The solvent is then distilled off in vacuo and the residue is dried in vacuo, giving 1473 g (97% of the theoretical) of 1-(3,5-dioxo-1,2,4-triazolidin-4-yl-methyl)-1,3,3-trimethyl-5-(3,5-dioxo-1,2,4-triazolidin-4-yl)-cyclohexane in the form of colourless crystals melting at 213 C. (decomposition). The solvent is then distilled off in vacuo the residue is dried in vacuo

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 131 g of 3-butoxy propylamine and 120 g of hydrazodicarbonamide are stirred in 300 ml of N-methyl pyrrolidone for 1 hour at 150° C., for 2 hours at 175° C. and for 6 hours at 200° C. A deposit is precipitated on cooling which is isolated by filtration under suction and recrystallised from cyclohexane, giving 152 g (75% of the theoretical yield) of 4-(3-butoxypropyl)-1,2,4-triazolidine-3,5-dione in the form of colourless crystals melting at 83° to 85° C. A deposit is precipitated on cooling which is isolated by filtration under suction recrystallised from cyclohexane giving 152 g (75% of the

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 360 g of hydrazodicarbonamide, 807 g of stearylamine and 1 ml of tin(II)dioctoate are stirred in 1 liter of N-methyl pyrrolidone for 4 hours at 175° C. and for 6 hours at 200° C. A deposit is precipitated on cooling and is filtered off under suction and washed with water, giving 955 g (90% of the theoretical yield) of 4-stearyl-1,2,4-triazolidine-3,5-dione in the form of colourless crystals melting at 118° to 120° C. A deposit is precipitated on cooling is filtered off under suction washed with water giving 955 g (90% of the

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 360 g of hydrazodicarbonamide, 807 g of stearylamine and 1 ml of tin(II)dioctoate are stirred in 1 liter of N-methyl pyrrolidone for 4 hours at 175° C. and for 6 hours at 200° C. A deposit is precipitated on cooling and is filtered off under suction and washed with water, giving 955 g (90% of the theoretical yield) of 4-stearyl-1,2,4-triazolidine-3,5-dione in the form of colourless crystals melting at 118° to 120° C. A deposit is precipitated on cooling is filtered off under suction washed with water giving 955 g (90% of the

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 360 g of hydrazodicarbonamide, 807 g of stearylamine and 1 ml of tin(II)dioctoate are stirred in 1 liter of N-methyl pyrrolidone for 4 hours at 175° C. and for 6 hours at 200° C. A deposit is precipitated on cooling and is filtered off under suction and washed with water, giving 955 g (90% of the theoretical yield) of 4-stearyl-1,2,4-triazolidine-3,5-dione in the form of colourless crystals melting at 118° to 120° C. A deposit is precipitated on cooling is filtered off under suction washed with water giving 955 g (90% of the